The objective of this project is research on and development of new mass spectral techniques in order to provide innovative and/or more rapid solutions to problems involving (1) chemical structure determination, (2) complex mixture analysis and (3) measurement of trace components in biological systems. Fast atom bombardment mass spectrometry and combined liquid chromatography-mass spectrometry remain the techniques of current interest. Both anion exchange and reverse phase microcolumn liquid chromatography have been combined with a continuous-flow fast atom bombardment ionization interface for the analysis of nucleosides, nucleotides and DNA adducts. Use of quaternary amine surfactants during static and continuous-flow fast atom bombardment greatly enhances sensitivity for analysis of nucleotides. Combined liquid chromatography-mass spectrometry with electrospray ionization has been employed for the successful structural confirmation of a novel mitomycin C-DNA intrastrand cross-link.